Process for rendering finely-divided catalytic nickel non-pyrophoric and stable.



UNITED STATES PATENT curren EDWIN CUNO KAYSER, OF CINCINNATI, OHIO, ASSIGNOR TO THE PROCTER A ND GAMBLE COMIRANY, OF CINCINNATI, OI-IIO, A CORPORATION OF OHIO.

rnocnss r03 IRENDERING FINELY-DIVIDED CATALYTIC AND STABLE.

NICKEL NoN-rYRoPHomc 1,001,279. No Drawing.

To all whom 'it may concern:

Be it known that I, EDWIN CUNo KAYSER, a subject of the King of Great Britain and now residing at the city of Cincinnati, 1n the county of Hamilton and State of Ohio, have invented a certain new and useful Process for Rendering Finely-Divided Catalytic Nickel N on-Pyro-phoric and Stable,

fofwhich the following is a full, clear, and

exact description. v

Finely divided nickel powder, such as is obtained by reducing a suitable nickel compound at elevated temperature in a current of hydrogen, and such as of late finds em-' ployment in various chemical processes as a so-called catalyzer, possesses well known pyrophoric tendencies. Even when the material has, at the end of the reduction-period, been permitted to thoroughly cool in an atmosphere of hydrogen, on withdrawal from the apparatus and consequent exposure to air, it is liable to spontaneous ignition or at least to a rapid rise in temperature, indicating fatal oxidation. Powders with such tendencies are different to handle even on the smallest scale, and it is readily understood that they do not meet industrial and commercial requirements. The same strictures in a measure ap ly to such preparations, as represent fine y divided nickel, dlifused among or deposited upon some inert materlal.

The objectof this invention is to greatly diminish or entirely suppress these pyrophoric tendencies without lnterference with catalytic energy, and the manner and method for bringing about this result is as follows: i

Nickel oxid, hydrate, or their equivalents, or inert materials, impregnated or coated with these compounds, are heated in a current of hydrogen in a suitable apparatus and in such manner and under such conditiors, as areknown'to effect reduction and to yield catalytic metal, a temperature of five hundred to six hundred degrees centigrade being preferably maintained. vAs

soon as reduction is judged complete, which will be the case when no more steam 1s evolved, a brisk. current of carbonlc acld is turned into the apparatus, meantime vmaintaining the former' temperature, This treatment is continued for a considerable Specification of Letters Patent. Patented Aug, .22" 1911, Applicationvfiled December 27, 1909. Serial No. 535,143.

time, varying from one to several hours, according to the volume of the gas current, construction and size of apparatus, and weight and nature of charge; it must in no case 'be'interrupted until the escaping gas proves no lonoer inflammable, and it shall be continued beyond that period for such time, as actual experiences prove desirable in each particular case. At the termination ,of such period the apparatus and the material contained therein are cooled more or less rapldly, according to provislons.

made toward that object, a mo-deratehcurrent of carbonic acid being maintained continuously through the apparatus to prevent the ingress of air.

When the apparatus and its contents have attained normal temperature, the gas mixrent may be discontinued, but the apparatus remains closed and the charge is not withdrawn for several hours, such period of quiescence assisting toward the desired end.

If the manipulation described has been carried out with proper care and with due consideration of existing circumstances, the metallic powder or metalliferous material thus prepared will remain perfectly cold on exposure to air and may thus be exposed for days without thereby losing any of its- '1 initial catalytic energy. Unsuitable deviation from the lines laid down makes itself perceptible by a corresponding deviation from the desired result. i v

What I claim as new, and of my invention and desire to secure by Letters Patent, is

1. The method of rendering finely divided nickel non-pyrophoric and stable in the air, which consists 1n subjecting it, ,at elevated temperature, to the prolonged action of ,carbomc acid gas and subsequently cooling" it in an atmosphere of carbonic. acld gas.-

2. The method of producing finely divided nickel, non-pyrophoric and stable in air,

which consists in reducing a nickel 'compound with hydrogen at a high temperature and thereafter, at elevated'temperature, subjecting the powder to the action of carbonic acid gas,:- and subsequently cooling in an atmosphere of carbonic acid gas.

3. The method of producing finely divided nickel, non-pyrophoric and stable in the air, which consists 1n reducing a nickel compound, at elevated temperature, -in a current of hydrogen and thereafter, while maintaining the temperature, submitting the-resulting metallic owder to" a current of carbonic acid gas an finally cooling in, an atmosphere of carbonic acid gas.

. 4. The method of rendering finely divided in subjecting such material, at elevatedtem erature, to the prolongedaction of carbonic v acid gas and subsequently cooling it in an atmosphere of carbonicacid gas. 5. The method of producing finely divided nickel, diffused through or deposited upon an inert refractory material, non-pyro'phoric and stable in'the 'air, which method consists in submitting such a material, impregnated or coated with a-' nickel compound, at elevated temperature, successively to a current of hydrogen and of carbonic acid gas and finally cooling itin-an atmosphere of carbonic acid gas.

6. Finely divided nickel, rendered nonpyrophoric and stable in the air by the prolonged action thereon of carbonic acid gasat elevated temperature and by subsequent nickel, di

7 Non-pyrophoric, stable, finely divided nickel, produced by submitting a nlckel comcooling in an atmosphere of carbonic acid pound at elevated temperature successively to a current of hydrogen and of carbonic acid gas and finally cooling in an atmosphere of carbonic acid gas.

8. Nonyrophoric, stable,

vated temperature, to the action of carbonic acid gas and finally cooled in an atmosphere ofcarbonic acid gas.

9. Non-pyro horic, stable, finely divided nickelydiifuse an indifferent material, obtainedby submittin such material, coated or impregnated wit a nickel compound, at elevated temperature, to the successive action of hydro-. gen and of carbonic acid gas and finally cooling in an atmosphere of carbonic acid as. g EDWIN CUNO KAYSER.

Witnesses: EARL W. GRIFFIN, MARSTO'N ALLEN.

35 finely divided used through or deposited upon "an indiflerent material, submitted, at elethrough or dep0s1ted upon 

